CN108896365A - A kind of lossless preparation method of transmission electron microscope in-situ mechanical sample - Google Patents
A kind of lossless preparation method of transmission electron microscope in-situ mechanical sample Download PDFInfo
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
A kind of lossless preparation method of transmission electron microscope in-situ mechanical sample,By sample dispersion in alcohol,Pt is deposited to the contact position of nano-machine hand and sample using the ion beam of 5-20pA,Manipulator and sample are welded,One end far from manipulator stretches out sample stage and forms cantilever beam,The length of cantilever beam is 500nm-5 μm,Sample is deposited with Pt with the ion beam of 5-30pA close to manipulator and fixes sample,Sedimentation time is 20-50s,Then manipulator probe tip is cut off using the ion beam of 100-600pA,Take out the in-situ mechanical test specimens sample platform for being placed with sample,Sample is fixed with epoxy resin conduction elargol using micro-mechanical device under an optical microscope,The in-situ mechanical sample stage for being fixed with sample is fixed on the specimen holder of transmission electron microscope in-situ mechanical system sample bar using conductive silver paint,Transmission electron microscope in-situ compression is carried out to sample under transmission electron microscope with tack pressing,It buckles and crooked experiment.
Description
Technical field
The present invention relates to one-dimensional material transmission electron microscope mechanics home position testing methods, the in particular to in-situ nano of one-dimensional material
Mechanical test belongs to transmission electron microscope in-situ nano mechanical test technical field.
Background technique
With the fast development of the great aerospace science and technology such as Aeronautics and Astronautics and deep space exploration, people equip high-performance
Requirement it is higher and higher, and high-performance equips and be unable to do without severe service components, therefore to the accuracy of manufacture and its performance of machine components
It is required that proposing a series of processing request of harshnesses.Generally the finished surface of severe service components is required to reach Subnano-class surface thick
Rugosity and nanometer-level plane degree, surface/sub-surface is not damaged, and traditional processing technology and equipment are difficult to meet such processing
It is required that and surface/sub-surface damage for generating often will affect the performance of part, substantially reduce service life to serious shadow
Ring the performance entirely equipped.In order to research and develop the Ultra-precision Turning technique and equipment that meet processing request, need to nano-precision table
The processing mechanism that wheat flour is made is studied.The essence of machining is exactly the removal material of the effect to material applied force, wherein from
The plastoelastic deformation mechanism of material is not opened, and transmission electron microscope in-situ mechanical method is the background science of research material deformation mechanism
Method.Mechanical test is combined with high-resolution-ration transmission electric-lens, by carrying out stress induced deformation on an atomic scale, in real time
The differentiation that ess-strain acts on lower material microstructure is recorded, intuitively discloses material in elasticity and the deformation machine of plastic stage
Reason.To provide theoretical and experiment basis to the great Ultra-precision Turning technique of research and development and equipment, to meet receiving for severe service components
Rice accuracy table wheat flour makes requirement.
Carry out the test of transmission electron microscope in-situ mechanical an important problem seek under small scale to sample " visible ",
" grabbing ", " drawing dynamic ", " measuring standard "." visible ", " grabbing " and " drawing dynamic " proposes the specimen material of test
Very high requirement.Sample in transmission electron microscope it is observed that, thickness cannot be greater than 150nm；And sample " will grab "
" drawing dynamic " just allows for effect that is fixed and withstanding forces.Monodimension nanometer material shows very big in these areas
Inherent advantage.The diameter of monodimension nanometer material is in nanoscale, and minimum is up to several nanometers, and its length arrives millimeter up to several microns
Magnitude.To can not only guarantee see under transmission electron microscope, but also it can guarantee the effect that sample is capable of fixing and withstands forces.This
Outer one-dimensional material itself is not necessarily to complicated working process, avoids bring damage and pollution in process.At present about one
Dimension nano material in situ TEM sample preparation methods mainly transfer the sample into sample in situ using FIB two-beam operating system
In sample platform and use the fixed sample of the method for ion beam depositing.This method during transfer and fixation with energy it is very big from
Beamlet can generate pollution and damage to nanotube sample, to the mechanical property of sample, electric property and micro-structural test and table
Sign is generated and is seriously affected.Therefore, it is necessary to research and develop the lossless preparation method of transmission electron microscope in-situ mechanical sample.
Summary of the invention
The present invention is different from traditional FIB method for making sample and generates ion beam pollution and damage and micromechanics dress to sample
The sample of nanoscale can not be operated by setting sample preparation, and the present invention provides a kind of the lossless of transmission electron microscope in-situ mechanical sample
Preparation method, and pollution of the FIB intermediate ion beam to sample is successfully avoided using FIB and micro-mechanical device by comprehensive
And damage.
Technical solution of the present invention：
A kind of lossless preparation method of transmission electron microscope in-situ mechanical sample, by sample dispersion in alcoholic solution, length
Range is 20-150 μm, diameter range 20-200nm.Pt is deposited into nano-machine hand and sample using the ion beam of 5-20pA
The contact position of product, manipulator and sample are welded, and one end far from manipulator stretches out sample stage and forms cantilever beam, cantilever
The length of beam is 500nm-5 μm, is deposited with the ion beam of 5-30pA with Pt in sample close to the place of manipulator and fixes sample,
Sedimentation time is 20-50s, is then cut off manipulator probe tip using the ion beam of 100-600pA, and taking-up is placed with sample
In-situ mechanical test specimens sample platform, sample is carried out with epoxy resin conduction elargol using micro-mechanical device under an optical microscope
It is fixed, the in-situ mechanical sample stage for being fixed with sample is fixed on transmission electron microscope in-situ mechanical system sample bar using conductive silver paint
Specimen holder on, transmission electron microscope in-situ compression is carried out to sample under transmission electron microscope with tack pressing, is buckled and crooked experiment.
Sample is nano wire, nanotube monodimension nanometer material.The diameter of monodimension nanometer material, not only can be in nanoscale
The work for directly observing the microstructure of material in transmission electron microscope, and being capable of fixing and withstanding forces in the longitudinal direction
With.Furthermore one-dimensional material itself, which is not necessarily to complicated working process, to avoid as the test sample of in situ TEM
Bring damage and pollution in process.Therefore monodimension nanometer material is ideal transmission electron microscope in-situ mechanical test specimens
Product.
By sample dispersion in alcoholic solution, and ultrasound 1-3min, it then will be dissolved with the wine of sample using plastic sprayer
Smart spray solution is on the transmission electron microscope copper mesh of no carbon film.There are commonly solvents as one kind for alcohol, imitate to the dispersion of sample
Fruit is good, therefore sample is placed on ultrasonic disperse in alcohol.Plastic sprayer will can be uniformly sprayed onto dissolved with the alcohol of sample
On copper mesh, keep the sample on copper mesh not easy to reunite, can more obtain single nanotube sample.
The copper mesh for being placed with sample is fixed on the mould loft floor of FIB two-beam operating system, searches out list with electron beam imaging
The sample of root, length range are 20-150 μm, diameter range 20-200nm.Electron beam imaging compares ion beam imaging, energy
It is relatively sharp to measure low and imaging, in order to avoid sample is polluted and damaged by ion beam, selection is found using electron beam imaging and closed
Suitable sample.
Manipulation FIB system nano-machine hand be close to sample, and finally with sample end thereof contacts.Provisioned in FIB
Nano-machine hand can be moved in three dimensions, and position precision is nanoscale；Make manipulator and one section of sample contacts
To provide the position of deposition Pt, and it also can reduce pollution of the ion beam to the sample other end.
Pt deposits to the contact position of nano-machine hand and sample using the ion beam of 5-20pA, sedimentation time 5-30s,
Manipulator and sample are welded.Ion beam using small line is the pollution in order to reduce ion beam to sample, furthermore greatly
The ion beam of line is easy directly to interrupt sample and cannot achieve welding.
Manipulator transfers the sample into in-situ mechanical sample stage substrate edge, and sample is close to one end of manipulator in sample
In sample platform, and one end far from manipulator stretches out sample stage and forms cantilever beam, and the length of cantilever beam is 500nm-5 μm.By sample
Stretch out one section of formation cantilever beam and be to carry out transmission electron microscope and buckle in situ experiment, while it is also ensured that ion beam operation area
Domain is far from Experimental Area, to avoid pollution and damage of the ion beam to sample observation region.
It is deposited with the ion beam of 5-30pA with Pt in sample close to the place of manipulator and fixes sample, sedimentation time is
20-50s is then cut off manipulator probe tip using the ion beam of 100-600pA.Use the fixed sample of the ion beam of small line
Product can reduce damage of the ion beam to sample, while stretch out sample stage in the fixed sample that will be far from the place close to manipulator
Observation portion avoids pollution of the ion beam to sample observation region.Due to sample when touching the ion beam of big line pole
It is flexible, therefore in order to guarantee that sample is intact, tool hand probe tip is cut off in selection.
The in-situ mechanical test specimens sample platform for being placed with sample is taken out, utilizes micro-mechanical device by sample under an optical microscope
It is fixed with epoxy resin conduction elargol, is placed 5-10 hours in drying cupboard, solidify epoxy resin conduction elargol.It is conventional
In FIB sample preparation operation it is maximum to the pollution of sample and damage be exactly big line ion beam depositing Pt fixation sample, in order to keep away
Exempt to the damage of sample and pollution in FIB welding process, the present invention is under an optical microscope used sample using micro-mechanical device
Epoxy resin conduction elargol is fixed, and fixed area can not only complete the final fixation of sample against sample edge of table, can be with
It prevents sample in situ in experimentation in the invisible region in the transmission electron microscope visual field, i.e. region on sample stage, bends,
As shown in Figure 1.
The in-situ mechanical sample stage for being fixed with sample is fixed on transmission electron microscope in-situ mechanical system sample using conductive silver paint
On the specimen holder of product bar.Conductive silver paint can be such that the fixation of sample stage and specimen holder is not detached from an experiment, without regard to
It excessively fastens and causes disassembly difficult.
Specimen holder is fixed on specimen holder using screw, transmission electricity is carried out to sample under transmission electron microscope with tack pressing
Mirror in-situ compression is buckled and crooked experiment.In order to apply pressure to sample, makes sample compression, buckles or be bent, use tack
Pressing is more easier to be pressed onto sample.
Detailed description of the invention
Fig. 1 is sample preparation methods schematic diagram of the invention.
Fig. 2 is the SEM figure for completing sample in FIB and fixing and cutting away manipulator probe tip.
Fig. 3 is the SEM figure after completing preparation.Grey column is sample, and a diameter of 75nm stretches out sample stage part
It is 4.2 μm, black portions are sample stage.
In figure：1 in-situ mechanical test specimens sample platform；2 deposit the region of Pt when fixing sample in FIB；3 monodimension nanometer materials
Sample；The position of 4 conductive silver glues when fixing sample in optical microscopy；5 samples stretch out 500nm-5 μm of sample stage formation
Cantilever beam.
Specific embodiment
The ZnO nano-wire for taking a little reunion shape, places it in alcoholic solution, and ultrasound 2min, is then sprayed using plastics
Sample is sprayed on copper mesh by day with fog, finally using alcohol extra on drying lamp removal copper mesh.
Then single sample is transferred in in-situ mechanical test specimens sample platform from copper mesh using FIB operating system.It will put
After thering is the copper mesh of sample to put FIB into, three single ZnO nano-wires are searched out with electron beam imaging, the first root long degree is 114 μm straight
Diameter is 70nm；It is 60nm that second root long degree, which is 110 μ m diameters,；It is 65nm that third root long degree, which is 85 μ m diameters,.Operate FIB system
Nano-machine hand is close to sample, and finally with sample end thereof contacts.Pt is deposited using the ion beam of the small line of 20pA
To the contact position of manipulator and sample, sedimentation time 20s welds manipulator and sample.Manipulator is by sample
Be transferred to in-situ mechanical sample stage substrate edge, guarantee sample close to one end of manipulator on sample stage, and far from manipulator
The other end stretch out sample stage and form cantilever beam, the length of cantilever beam is 4.5 μm.In sample close to the place 30pA of manipulator
The ion beam of small line sample is fixed, sedimentation time 40s then cuts away manipulator using the big line of 300pA
Probe tip, as illustrated in fig. 1 and 2.Successfully ZnO nano-wire is transferred on in-situ test sample stage from copper mesh, avoid from
Pollution and damage of the beamlet to sample.
The in-situ test sample stage for being placed with ZnO nano-wire is taken out, is placed under an optical microscope.It is dipped in accurate operation hand
Extracting epoxy resin conductive silver glue drips on sample, fixes sample with in-situ test sample stage.The original position of ZnO nano-wire will be placed with
Test specimens sample platform is placed 8 hours in drying cupboard, solidifies elargol.
After completing solidification, the sample stage for being fixed with sample is fixed on transmission electron microscope in-situ nano mechanics using conductive silver paint
On the specimen holder of system sample bar.Then specimen holder is screwed on specimen holder, transmission electron microscope in-situ mechanical is completed and surveys
Test agent preparation process, as shown in Figure 3.The sample of preparation can be used for transmission electron microscope in-situ compression, buckle and crooked experiment.
Claims (1)
1. a kind of lossless preparation method of transmission electron microscope in-situ mechanical sample, in-situ compression is carried out in transmission electron microscope, buckle and
Crooked experiment, it is characterised in that：
(1) sample is nano wire, nanotube monodimension nanometer material；
(2) by sample dispersion in alcohol, and ultrasound 1-3min, it then will be dissolved with the alcoholic solution of sample using plastic sprayer
It is sprayed on the transmission electron microscope copper mesh of no carbon film；
(3) the transmission electron microscope copper mesh for being placed with sample is fixed on the mould loft floor of FIB two-beam operating system, is sought with electron beam imaging
Single sample is found, length range is 20-150 μm, diameter range 20-200nm；
(4) manipulate FIB two-beam operating system nano-machine hand be close to sample, and finally with sample end thereof contacts；
(5) Pt deposits to the contact position of nano-machine hand and sample using the ion beam of 5-20pA, sedimentation time 5-30s,
Manipulator and sample are welded；
(6) manipulator transfers the sample into in-situ mechanical test sample platform substrate edge, and sample is close to one end of manipulator
On sample stage, one end far from manipulator stretches out sample stage and forms cantilever beam, and the length of cantilever beam is 500nm-5 μm；
(7) it is deposited with the ion beam of 5-30pA by Pt at manipulator in sample and fixes sample, sedimentation time 20-
50s is then cut off manipulator probe tip using the ion beam of 100-600pA；
(8) the in-situ mechanical test specimens sample platform for being placed with sample is taken out, utilizes micro-mechanical device by sample under an optical microscope
It is fixed with epoxy resin conduction elargol, is placed 5-10 hours in drying cupboard, solidify epoxy resin conduction elargol；
(9) the in-situ mechanical test specimens sample platform for being fixed with sample is fixed on transmission electron microscope in-situ mechanical system using conductive silver paint
On the specimen holder of specimen holder；
(10) specimen holder is fixed on specimen holder using screw, transmission electricity is carried out to sample under transmission electron microscope with tack pressing
Mirror in-situ compression is buckled and crooked experiment.
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| CN201810734397.5A CN108896365B (en) | 2018-07-06 | 2018-07-06 | Nondestructive preparation method of transmission electron microscope in-situ mechanical sample |
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Cited By (8)
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| CN109827820A (en) * | 2019-03-07 | 2019-05-31 | 中国工程物理研究院材料研究所 | A kind of in situ TEM sample preparation methods based on heating chip |
| CN110057851A (en) * | 2019-05-17 | 2019-07-26 | 中国科学院地球化学研究所 | A method of the multiple TEM chip samples of micron-sized individual particle are prepared in situ |
| CN110596427A (en) * | 2019-08-15 | 2019-12-20 | 南京理工大学 | Method for preparing three-dimensional atom probe sample on powder particles |
| CN111474197A (en) * | 2020-04-16 | 2020-07-31 | 宸鸿科技(厦门)有限公司 | Method for controlling contamination resulting from transmission electron microscope sample preparation |
| CN113340926A (en) * | 2020-03-03 | 2021-09-03 | 中国科学院物理研究所 | Sample transfer method of chip type in-situ transmission electron microscope |
| CN114166674A (en) * | 2021-12-03 | 2022-03-11 | 中国地质大学（北京） | Test device and method for metal surface interface abrasion |
| US11313774B2 (en) * | 2018-04-18 | 2022-04-26 | Dalian University Of Technology | TEM electromechanical in-situ testing method of one-dimensional materials |
| CN115684229A (en) * | 2022-09-21 | 2023-02-03 | 哈尔滨工业大学 | Preparation method of micron-sized particle section capable of being repeatedly used for electron microscope observation |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US11313774B2 (en) * | 2018-04-18 | 2022-04-26 | Dalian University Of Technology | TEM electromechanical in-situ testing method of one-dimensional materials |
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| CN111474197A (en) * | 2020-04-16 | 2020-07-31 | 宸鸿科技(厦门)有限公司 | Method for controlling contamination resulting from transmission electron microscope sample preparation |
| CN114166674A (en) * | 2021-12-03 | 2022-03-11 | 中国地质大学（北京） | Test device and method for metal surface interface abrasion |
| CN114166674B (en) * | 2021-12-03 | 2024-01-30 | 中国地质大学（北京） | Device and method for testing interface abrasion of metal surface |
| CN115684229A (en) * | 2022-09-21 | 2023-02-03 | 哈尔滨工业大学 | Preparation method of micron-sized particle section capable of being repeatedly used for electron microscope observation |
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